Manufacturing method of semi-insulating single-crystal silicon carbide powder

ABSTRACT

The present disclosure provides a manufacturing method of semi-insulating single-crystal silicon carbide powder comprising: providing a semi-insulating single-crystal silicon carbide bulk, wherein the semi-insulating single-crystal silicon carbide bulk has a first silicon-vacancy concentration, and the first silicon-vacancy concentration is greater than 5E11 cm{circumflex over ( )}−3; refining the semi-insulating single-crystal silicon carbide bulk to obtain a semi-insulating single-crystal silicon carbide coarse particle, wherein the semi-insulating single-crystal silicon carbide coarse particle has a second silicon-vacancy concentration and a first particle diameter, the second silicon-vacancy concentration is greater than 5E11 cm{circumflex over ( )}−3, and the first particle diameter is between 50 μm and 350 μm; self-impacting the semi-insulating single-crystal silicon carbide coarse particle to obtain a semi-insulating single-crystal silicon carbide powder, wherein the semi-insulating single-crystal silicon carbide powder has a third silicon-vacancy concentration and a second particle diameter, the third silicon-vacancy concentration is greater than 5E11 cm{circumflex over ( )}−3, and the second particle diameter is between 1 μm and 50 μm.

CROSS REFERENCE TO RELATED DISCLOSURE

This application claims the priority benefit of Taiwan PatentApplication Number 110101834, filed on Jan. 18, 2021 and Taiwan PatentApplication Number 109120678, filed on Jun. 18, 2020, the fulldisclosure of which are incorporated herein by reference.

BACKGROUND Technical Field

The application relates to the technical field of a manufacturing methodof silicon carbide powder, particularly to a manufacturing method ofsemi-insulating single-crystal silicon carbide powder with highsilicon-vacancy concentration.

Related Art

Semiconductor materials have gone through three stages of development.The first generation is about basic functional materials of silicon(Si), germanium (Ge), etc.; the second generation is about compoundsemiconductor materials composed of two or more elements, whereingallium arsenide (GaAs), indium phosphide (InP), etc. arerepresentative; the third generation is about compound semiconductormaterials such as gallium nitride (GaN) and silicon carbide (SiC). Thesemiconductor materials of the third generation are materials with wideenergy band gaps, which have the advantages of high frequency, highvoltage resistivity, and high-temperature resistivity. The semiconductormaterials of the third generation have good electrical conductivity andheat dissipation to reduce energy consumption. The volume of elementscomprised the semiconductor materials of the third generation isrelatively small, thereby suitable for power semiconductor applications.However, controlling the production conditions of silicon carbide isdifficult, which makes the mass production of silicon carbide wafersdifficult. Thereby, the development of terminal wafers and applicationsis affected directly.

On the other hand, in addition to being used as a wafer in thesemiconductor industry, silicon carbide materials can also be used asfluorescent materials in the biomedical industry. For example,semi-insulating single-crystal silicon carbide has luminescencecharacteristics and can be used as a tracking detection target. However,the luminescence characteristics are affected by the surface morphologyof the silicon carbide powder. In this case, the silicon carbide powderobtained by the wet process (for example, using diamond wire cutting)has a rough surface and is easily doped with impurities. The particlesize may even be increased due to agglomeration. As a result, theluminous efficiency of the silicon carbide powder will be sharplyreduced. Therefore, achieving a stable luminous effect is difficult.

SUMMARY

Given the defect of the above-mentioned prior art, the presentapplication provides a manufacturing method of silicon carbide powder,particularly to a manufacturing method of semi-insulating single-crystalsilicon carbide powder with high silicon-vacancy concentration.

According to a manufacturing method of semi-insulating single-crystalsilicon carbide powder disclosed in the embodiments of the presentapplication, the manufacturing method includes: providing asemi-insulating single-crystal silicon carbide bulk, wherein thesemi-insulating single-crystal silicon carbide bulk has a firstsilicon-vacancy concentration, and the first silicon-vacancyconcentration is greater than 5E11 cm{circumflex over ( )}−3; refiningthe semi-insulating single-crystal silicon carbide bulk to obtain asemi-insulating single-crystal silicon carbide coarse particle, whereinthe semi-insulating single-crystal silicon carbide coarse particle has asecond silicon-vacancy concentration and a first particle diameter, thesecond silicon-vacancy concentration is greater than 5E11 cm{circumflexover ( )}−3, and the first particle diameter is between 50 μm and 350μm; self-impacting the semi-insulating single-crystal silicon carbidecoarse particle to obtain a semi-insulating single-crystal siliconcarbide powder, wherein the semi-insulating single-crystal siliconcarbide powder has a third silicon-vacancy concentration and a secondparticle diameter, the third silicon-vacancy concentration is greaterthan 5E11 cm{circumflex over ( )}−3, and the second particle diameter isbetween 1 μm and 50 μm.

Other advantages of the present application will be explained in moredetail with the following descriptions and figures.

It should be understood, however, that this summary may not contain allaspects and embodiments of the present invention, that this summary isnot meant to be limiting or restrictive in any manner, and that theinvention as disclosed herein will be understood by one of ordinaryskill in the art to encompass obvious improvements and modificationsthereto.

BRIEF DESCRIPTION OF THE DRAWINGS

The figures described herein are used to provide a further understandingof the application and constitute a part of the application. Theexemplary embodiments and descriptions of the application are used toillustrate the application and do not limit the application, in which:

FIG. 1 is a schematic diagram of the growth system for growinghigh-purity semi-insulating single-crystal silicon carbide crystalaccording to the present application;

FIG. 2 is a measurement result of the resistivity of the high-puritysemi-insulating single-crystal silicon carbide crystal according to thefirst embodiment of the present application;

FIG. 3 is a schematic diagram of the micro-pipe density of thehigh-purity semi-insulating single-crystal silicon carbide crystalaccording to the first embodiment of the present application;

FIG. 4 is an electron paramagnetic resonance spectrum of the high-puritysemi-insulating single-crystal silicon carbide crystal according to thefirst embodiment of the present application;

FIG. 5 is a measurement result of the resistivity of the high-puritysemi-insulating single-crystal silicon carbide crystal according to thesecond embodiment of the present application;

FIG. 6 is a schematic diagram of the micro-pipe density of thehigh-purity semi-insulating single-crystal silicon carbide crystalaccording to the second embodiment of the present application;

FIG. 7 is an electron paramagnetic resonance spectrum of the high-puritysemi-insulating single-crystal silicon carbide crystal according to thesecond embodiment of the present application;

FIG. 8 is a schematic diagram of the silicon-vacancy concentration ofthe silicon carbide wafer according to the second embodiment of thepresent application;

FIG. 9 is a photoluminescence spectrum of a silicon carbide waferaccording to the second embodiment of the present application;

FIG. 10 is a photoluminescence spectrum of a silicon carbide waferaccording to the second embodiment of the present application;

FIG. 11 is a schematic diagram of the PL/TO ratio according to the firstembodiment of the present application;

FIG. 12 is a schematic diagram of the micro-pipe density of thehigh-purity semi-insulating single-crystal silicon carbide waferaccording to the third embodiment of the present application;

FIG. 13 is a schematic diagram of the micro-pipe density of thehigh-purity semi-insulating single-crystal silicon carbide waferaccording to the fourth embodiment of the present application;

FIGS. 14 to 17 are respectively schematic diagrams of thesilicon-vacancy concentration of each slice of the semi-insulatingsingle-crystal silicon carbide bulk material according to the fifthembodiment of the present application;

FIG. 18 is a schematic diagram of the processing of the semi-insulatingsingle-crystal silicon carbide powder of the sixth embodiment of thepresent application;

FIG. 19 is a schematic diagram of the silicon-vacancy concentration ofthe semi-insulating single-crystal silicon carbide residue according tothe sixth embodiment of the present application;

FIG. 20 is a schematic diagram of the silicon-vacancy concentration ofeach slice of the semi-insulating single-crystal silicon carbide residueof the sixth embodiment of the present application;

FIG. 21 is a schematic diagram of the relationship between thewavelength and the luminous intensity of the semi-insulatingsingle-crystal silicon carbide powder according to the sixth embodimentof the present application;

FIG. 22 is a flow chart of the manufacturing method of semi-insulatingsingle-crystal silicon carbide powder according to the seventhembodiment of the present application;

FIG. 23 is a particle size analysis diagram of the semi-insulatingsingle-crystal silicon carbide coarse particle according to the eighthembodiment of the present application; and

FIGS. 24-29 are respectively particle size analysis diagrams of thesemi-insulating single-crystal silicon carbide powder according to theeighth embodiment of the present application.

DETAILED DESCRIPTION OF THE EMBODIMENTS

In order to make the objectives, technical solutions, and advantages ofthe present application more clear, the technical solutions of theapplication will be described clearly and completely in conjunction withspecific embodiments and the figures of the application. Obviously, thedescribed embodiments are only a part of the embodiments of theapplication, rather than all the embodiments. Based on the embodimentsin the application, all other embodiments obtained by a person ofordinary skill in the art without creative work fall within theprotection scope of this disclosure.

The following description is of the best-contemplated mode of carryingout the invention. This description is made for the purpose ofillustrating the general principles of the invention and should not betaken in a limiting sense. The scope of the invention is best determinedby reference to the appended claims.

Certain terms are used throughout the description and following claimsto refer to particular components. As one skilled in the art willappreciate, manufacturers may refer to a component by different names.This document does not intend to distinguish between components thatdiffer in name but function. “Substantial/substantially” means, withinan acceptable error range, the person skilled in the art may solve thetechnical problem in a certain error range to achieve the basictechnical effect.

Moreover, the terms “include”, “contain”, and any variation thereof areintended to cover a non-exclusive inclusion. Therefore, a process,method, object, or device that comprises a series of elements not onlyinclude these elements, but also comprises other elements not specifiedexpressly, or may include inherent elements of the process, method,object, or device. If no more limitations are made, an element limitedby “include a/an . . . ” does not exclude other same elements existingin the process, the method, the article, or the device which comprisesthe element.

In the following embodiment, the same reference numerals are used torefer to the same or similar elements throughout the invention.

The present application discloses a high-purity semi-insulatingsingle-crystal silicon carbide bulk material with large-size,high-resistivity, and low-defect, which is grown in a high-puritysingle-crystal system by physical vapor transport (PVT). By controllingthe Si/C ratio and particle size distribution of the high-purity crystalgrowth raw material, and the crystal growth temperature and time duringthe crystal growth process, the system becomes a carbon-rich (C-rich)environment. In a state where shallow-level conductive elements arescarce, the intrinsic defect of silicon vacancy may be generated in thecrystal and the silicon-vacancy concentration may be controlled. Theintrinsic defect is used to increase the resistivity of the crystal inorder to make the wafer semi-insulate. In addition, the possibility ofintroducing impurities into the crystal is eliminated during the crystalgrowth process due to the high-purity raw material. Therefore, thepresent application discloses a high-purity semi-insulatingsingle-crystal silicon carbide bulk material with a micro-pipe defectless than 3 cm{circumflex over ( )}−2.

“Large size” mentioned here refers to a high-purity semi-insulatingsingle-crystal silicon carbide wafer with a diameter of at least 4inches, or 4 inches to 6 inches, and a thickness of at least 350 μm.“High purity” refers to the purity of the raw material used for growncrystal is higher than 99.99%. “High resistivity” refers to theresistivity is greater than 1E7 ohm-cm or at least 1E7 ohm-cm at roomtemperature. In addition, the crystal refers to a silicon carbidecrystal manufactured by a silicon carbide growth system in theembodiments of the specification, and the finished product after cuttingthe silicon carbide crystal is generally called wafer.

The high resistivity characteristic of the high-purity semi-insulatingsingle-crystal silicon carbide crystal or silicon carbide wafer of thepresent application is controlled by the concentration of intrinsicdefect (silicon vacancy) in the crystal or wafer. The silicon vacancy isgenerated during the crystal growth process. An additional annealingprocess or neutron bombardment process is unnecessary therebysimplifying the manufacturing process.

Refer to FIG. 1, which is a schematic diagram of the growth system forgrowing high-purity semi-insulating single-crystal silicon carbidecrystal according to the present application. As shown in the figure,the growth system comprises a crucible 2, a thermal insulation material3, and a heater 7. The crucible 2 is used to contain a seed 1 whichgrows through a material source 6. The thermal insulation material 3 isdisposed on the outside of the crucible 2. The thermal insulationmaterial 3 shown in the figure covers the outside of the crucible 2, butthe thermal insulation material 3 does not have to substantially coverthe outside of the crucible 2, as long as the temperature may bemaintained. Therefore, the figure is only exemplary. The heater 7 isused to provide a heat source. The number of the heater 7 shown in thefigure is multiple, but the number of the heater 7 may also be providedin one depending on the system configuration. The number of the heater 7in the figure is only for the purposes of exemplary and does not limitthe real number of heater 7. A high-frequency heater or a resistivityheater may be used as the heater 7. In a more specific embodiment, aheating coil or heating resistivity wire (net) may be used as the heater7.

A holder 4 is disposed above the inside of the crucible 2, and theholder 4 is used to fix the seed 1. The material source 6 may bedisposed below the crucible 2, and the space between the seed 1 and thematerial source 6 may be used as a growth area 5 for silicon carbidecrystal. The area where the seed 1 is placed may be defined as the seedarea, and the area where the material source 6 is placed may be definedas the material source area. Therefore, the empty crucible 2 has a seedarea, a material source area, and a growth area inside. In anon-limiting embodiment, the crucible 2 may be a graphite crucible, andthe thermal insulation material 3 may be a graphite blanket or a porousthermal insulation carbon material.

In the embodiment, the seed may be silicon carbide. The seed used in thepresent application may be a single-crystal wafer with a thickness of350 μm or more and a diameter of 4 inches to 6 inches or more to grow asingle-crystal with the corresponding size or more. The single-crystalwafer may be silicon carbide. The material source area in the cruciblemay be silicon carbide. The material source may be powdery, granular, ormassive and have a purity of more than 99.99%. The crystalline phase ofthe material source may be α or β, and the ratio of silicon/carbon maybe 0.95 to 1.05.

By controlling the temperature distribution, the atmosphere flow, andthe sublimation process of the material source in the crucible 2 withthe structure of the crucible 2, the structure of the thermal-material3, and the heater 7, the sublimated gas molecules are transported anddeposited on the seed 1 (wafer) to generate silicon carbide crystal. Inan embodiment of the growth process, the temperature difference betweenthe bottom of the crucible to the seed area is controlled in the rangeof 10° C. to 300° C., the flow rate of argon gas is controlled in therange of 100 sccm to 1000 sccm, the pressure is controlled in the rangeof 1 torr to 200 torrs, and the temperature range of the seed duringcrystallization is controlled between 2000° C. and 2270° C. Controllingthe purity and type of the material source, and the temperature rangeand time of growth are the most important. After the conductive elementsinside the system are consumed, the electrical performance of thecrystal may be majorly dominated by the intrinsic defect generatedinside the crystal.

The high-purity semi-insulating single-crystal silicon carbide crystalformed by the growth system of the above embodiment is grown bydepositing a vapor material containing Si and C on the surface of theseed. The high-purity semi-insulating single-crystal silicon carbidecrystal comprises one polytype single-crystal. The high-puritysemi-insulating single-crystal silicon carbide crystal has siliconvacancy inside, wherein the silicon-vacancy concentration is at leastgreater than 5E11 cm{circumflex over ( )}−3 and less than 5E13cm{circumflex over ( )}−3. In the prior art, the concentration ofsilicon vacancy in silicon carbide wafer is about 2E11 cm{circumflexover ( )}−3 to 3E11 cm{circumflex over ( )}−3 generally.

In one embodiment, the high-purity semi-insulating single-crystalsilicon carbide crystal formed by the growth system according to theabove embodiment has a diameter greater than or equal to 90 mm.

In one embodiment, the diameter of the high-purity semi-insulatingsingle-crystal silicon carbide crystal formed by the growth systemaccording to the above embodiment is less than or equal to 200 mm.

In one embodiment, the high-purity semi-insulating single-crystalsilicon carbide crystal formed by the growth system according to theabove embodiment has a resistivity greater than 1E7 ohm-cm.

In one embodiment, the high-purity semi-insulating single-crystalsilicon carbide crystal formed by the growth system according to theabove embodiment has a micro-pipe density of less than 3 per squarecentimeter.

In one embodiment, the high-purity semi-insulating single-crystalsilicon carbide crystal formed by the growth system according to theabove embodiment has a micro-pipe density of less than 2 per squarecentimeter.

In one embodiment, the high-purity semi-insulating single-crystalsilicon carbide crystal formed by the growth system according to theabove embodiment has a micro-pipe density of less than 1 per squarecentimeter.

In one embodiment, the high-purity semi-insulating single-crystalsilicon carbide crystal formed by the growth system according to theabove embodiment has a micro-pipe density of less than 0.4 per squarecentimeter.

In one embodiment, the high-purity semi-insulating single-crystalsilicon carbide crystal formed by the growth system according to theabove embodiment has a micro-pipe density of less than 0.1 per squarecentimeter.

In one embodiment, the high-purity semi-insulating single-crystalsilicon carbide crystal formed by the growth system according to theabove embodiment comprises one polytype single-crystal selected from 3C,4H, 6H, and 15R polymorphs of silicon carbide, wherein the 4H polymorphis the most preferred currently. The wafer may be selected from 3C, 4H,6H, and 15R polymorphs of silicon carbide, wherein the 4H polymorph isthe most preferred currently. The wafer obtained is oriented along anaxis, such as a positive axis orientation, or a variety of off-axisorientations. For example (but not limited to), the wafer is selectedfrom 4°, 3.5°, and 2°.

In one embodiment, the thickness of the high-purity semi-insulatingsingle-crystal silicon carbide crystal formed by the growth systemaccording to the above embodiment is at least 8 mm.

In one embodiment, the thickness of the high-purity semi-insulatingsingle-crystal silicon carbide crystal formed by the growth systemaccording to the above embodiment is 8 mm to 30 mm.

The following embodiment illustrates the specific manufacturing processof the high-purity semi-insulating single-crystal silicon carbidecrystal disclosed in the present application. Through physical vaportransport (PVT), using high-purity growth materials and components, andadjusting process window and time, the manufacturing process is not onlyeffectively inhibiting impurities and conductive elements from enteringthe crystal during the crystal growth process but improving the qualityof the crystal. By thermal field optimization and process control, theoverall crystal growth surface is flatter, and the intrinsic defectconcentration of the crystal is increased. Thereby, the resistivity of1E7 ohm-cm of the silicon carbide crystal with 4 to 6 inches isachieved.

The first embodiment illustrates growing a 6-inch single-crystal siliconcarbide crystal by using the growth system of FIG. 1. The material usedin the present embodiment is high-purity silicon carbide powder with apurity of 99.99% or more. The average particle size is 5 mm to 20 mm.The initial silicon/carbon ratio is 1. After the crystal growing, thesilicon/carbon ratio of the remaining material drops to 0.85.

The 4H—SiC single-crystal is manufactured by the PVT method with theabove-mentioned silicon carbide source. The growth process is performedin a graphite crucible in a high-temperature vacuum induction furnace.The growth temperature of the seed is about 2100° C. Ar is used as thecarrier gas for the system. The pressure during crystal growth of thesystem is about 5 torr, and the growth time is 150 hours. A siliconcarbide single crystal wafer of about 500 μm is used as a seed.

First, perform an air extraction process, and fix the 4H—SiC seed with aholder. Then, extract air to remove air and other impurities in thecrucible system. After extracting the air, perform a heating process.During the heating process, add the inert gas Ar as auxiliary gas, anduse the heating coil to heat the entire system. Heat to about 2100° C.and continually grow for up to 150 hours. Through the process conditionsof the first embodiment, a 6-inch single-crystal silicon carbide boulewith a convex interface shape may be produced, and the crystal growthrate may achieve 100-250 μm/hr.

The resistivity, micro-pipe density, impurity elements, or siliconvacancy of the crystal after growing may be measured. The crystal aftergrowing is sliced and polished to obtain a wafer. The wafer may bemeasured for resistivity without annealing. An area with a diameter of140 mm at the center of the 6-inch wafer is measured, the resistivityvalues are all greater than 1E7 ohm-cm, as shown in FIG. 2.

Analyze the 6-inch wafer with X-ray topography. As the result, thenumber of micro-pipes is 10. Furthermore, the overall density of 6-inchmicro-pipes is the number of micro-pipes/6 inch wafer area, which is10/(7.5*7.5*3.1416)=10/176.75=0.056. That is, the micro-pipe density inthis embodiment is less than 0.1 per square centimeter, as shown in FIG.3.

Analyze the impurity elements of the 6-inch wafer with Glow DischargeMass Spectrometer (GDMS) and Secondary Ion Mass Spectroscopy (SIMS), theresults of the following table may be obtained. Wherein, the N elementis measured by SIMS, and other elements are measured by GDMS. Two unitsof ppm and ion concentration are provided. The content of conductiveimpurity elements in the crystal is less than 5E15 cm{circumflex over( )}−3.

Crystal number Example 1 element GDMS (ppm/cm^(∧)−3) N SIMS: 4.30E+15 B  0.02 (3.76E+15) Al   0.04 (2.87 E+15) P <0.05 (<3.14E+15) Ti <0.01(<4.04E+14) V <0.01 (<3.38E+14) Fe  <0.1 (<3.46E+15) Ni <0.05(<1.67E+15)

Analyze the 6-inch wafer with the electron paramagnetic resonance (EPR).The spectroscopy shows that the main defect in the crystal is siliconvacancy. As shown in FIG. 4, the results of the optical inspection areused to show the silicon-vacancy concentration. The silicon-vacancyconcentration is from 5.22E11 cm{circumflex over ( )}−3 to 1.02E12cm{circumflex over ( )}−3.

The second embodiment illustrates growing a 4-inch single-crystalsilicon carbide boule by using the growth system of FIG. 1. The materialused in the present embodiment is high-purity silicon carbide powderwith a purity of 99.99% or more. The average particle size is 100 mm to30 mm. The initial silicon/carbon ratio is 1. After the crystal growing,the silicon/carbon ratio of the remaining material drops to 0.87.

The 4H—SiC single-crystal is manufactured by the PVT method with theabove-mentioned silicon carbide source. The growth process is performedin a graphite crucible in a high-temperature vacuum induction furnace.The growth temperature of the seed is about 2180° C. Ar is used as thecarrier gas for the system. The pressure during crystal growth of thesystem is about 5 torr, and the growth time is 200 hours. A siliconcarbide single crystal wafer of about 500 μm is used as a seed.

First, perform an air extraction process, and fix the 4H—SiC seed with aholder. Then, extract air to remove air and other impurities in thecrucible system. After extracting the air, perform a heating process.During the heating process, add the inert gas Ar as auxiliary gas, anduse the heating coil to heat the entire system. Heat to about 2100° C.and continually grow for up to 150 hours. Through the process conditionsof the first embodiment, a 6-inch single-crystal silicon carbide boulewith a convex interface shape may be produced, and the crystal growthrate may achieve 100-250 μm/hr.

The resistivity, micro-pipe density, impurity elements, or siliconvacancy of the crystal after growing may be measured. The crystal aftergrowing is sliced and polished to obtain a wafer. The wafer may bemeasured for resistivity without annealing. An area with a diameter of140 mm at the center of the 6-inch wafer is measured, the resistivityvalues are all greater than 1E7 ohm-cm, as shown in FIG. 5.

Analyze the 6-inch wafer with X-ray topography. As the result, thenumber of micro-pipes is 1. Furthermore, the overall density of 4-inchmicro-pipes is the number of micro-pipes/4 inch wafer area, which is1/(5*5*3.1416)=1/78.54=0.012. That is, the micro-pipe density in thisembodiment is less than 0.02 per square centimeter, as shown in FIG. 6.

Analyze the impurity elements of the 6-inch wafer with Glow DischargeMass Spectrometer (GDMS) and Secondary Ion Mass Spectroscopy (SIMS), theresults of the following table may be obtained. Wherein, the N elementis measured by SIMS, and other elements are measured by GDMS. Two unitsof ppm and ion concentration are provided. The content of conductiveimpurity elements in the crystal is less than 5E15 cm{circumflex over( )}−3.

Crystal number Example 2 element GDMS (ppm/cm^(∧)−3) N SIMS: 1.90E+15 B  0.04 (6.93E+15) Al   0.03 (2.10E+15) P <0.05 (<3.14E+15) Ti <0.01(<4.04E+14) V <0.01 (<3.38E+14) Fe  <0.1 (<3.46E+15) Ni <0.05(<1.67E+15)

Analyze the 4-inch wafer with the electron paramagnetic resonance (EPR).The spectroscopy shows that the main defect in the crystal is siliconvacancy. As shown in FIG. 7, the results of the optical inspection areused to show the silicon-vacancy concentration. The silicon-vacancyconcentration is 7.07E12 cm{circumflex over ( )}−3.

Cut the crystal of the second embodiment, and analyze thesilicon-vacancy concentration of the slices at different positions, asshown in FIG. 8. Taking the growth system of FIG. 1 as an example, atotal of 20 slices are cut, and the 20 slices respectively correspondingto the serial number on the horizontal axis of FIG. 8. Wherein theserial number of the slice closest to the seed is 1. From the seed tothe growth surface, the silicon-vacancy concentrations respectively are1.9E12 cm{circumflex over ( )}−3, 7E12 cm{circumflex over ( )}−3, 5.9E12cm{circumflex over ( )}−3, and 3.3 E12 cm{circumflex over ( )}−3,respectively.

The high-purity semi-insulating single-crystal silicon carbide waferaccording to the above embodiment comprises one polytype single-crystal.The high-purity semi-insulating single-crystal silicon carbide wafer hassilicon vacancy inside, wherein the silicon-vacancy concentration is atleast greater than 5E11 cm{circumflex over ( )}−3, less than 5E13cm{circumflex over ( )}−3.

In one embodiment, the high-purity semi-insulating single-crystalsilicon carbide wafer formed according to the above embodiment has adiameter greater than or equal to 90 mm.

In one embodiment, the diameter of the high-purity semi-insulatingsingle-crystal silicon carbide wafer formed according to the aboveembodiment is less than or equal to 200 mm.

In one embodiment, the high-purity semi-insulating single-crystalsilicon carbide wafer formed according to the above embodiment has aresistivity greater than 1E7 ohm-cm.

In one embodiment, the high-purity semi-insulating single-crystalsilicon carbide wafer formed according to the above embodiment has amicro-pipe density of less than 3 per square centimeter.

In one embodiment, the high-purity semi-insulating single-crystalsilicon carbide wafer formed according to the above embodiment has amicro-pipe density of less than 2 per square centimeter.

In one embodiment, the high-purity semi-insulating single-crystalsilicon carbide wafer formed according to the above embodiment has amicro-pipe density of less than 1 per square centimeter.

In one embodiment, the high-purity semi-insulating single-crystalsilicon carbide wafer formed according to the above embodiment has amicro-pipe density of less than 0.4 per square centimeter.

In one embodiment, the high-purity semi-insulating single-crystalsilicon carbide wafer formed according to the above embodiment has amicro-pipe density of less than 0.1 per square centimeter.

In one embodiment, the high-purity semi-insulating single-crystalsilicon carbide wafer formed according to the above embodiment comprisesone polytype single-crystal selected from 3C, 4H, 6H, and 15R polymorphsof silicon carbide, wherein the 4H polymorph is the most preferredcurrently. The wafer may be selected from 3C, 4H, 6H, and 15R polymorphsof silicon carbide, wherein the 4H polymorph is the most preferredcurrently. The wafer obtained is oriented along an axis, such as apositive axis orientation, or a variety of off-axis orientations. Forexample (but not limited to), the wafer is selected from 4°, 3.5°, and2°.

The wafer according to the present application is suitable forhigh-frequency power devices, high-power devices, high-temperaturedevices, optoelectronic devices, and deposition of group III nitrides.

The wafer according to the present application is suitable as asingle-photon light source, that is, an integrated circuit substrate ofa quantum computer.

Refer to FIG. 7, the electron paramagnetic resonance (EPR) spectrum ofthe second embodiment is shown. The sample was cut into a size of 5.5cm×7 mm and irradiated with a microwave of 9.70396×1E9 Hz. In thespectrum, the silicon carbide wafer produces a zero point at 3600.70343Gat a temperature of 300K. After calculation by the formula hυ=gμ_(B)B(h: Planck's constant, υ: frequency; g: g factor; μ_(B): Bohr magneton;B: magnetic field), the g factor of the No. 11 wafer of Example 2 is2.00343. It means that the silicon vacancy is contained in siliconcarbide (the signal of silicon vacancy is g=2.0032±0.0004).

Refer to FIG. 10, which is the photoluminescence spectrum of the waferof the second embodiment. Some Raman signals are not sensitive to theconcentration of doping and the concentration of vacancy, for example,lateral-optical mode. For laser excitation of 785 nm, it is the LO modeat the 851 nm wavelength and the 4H—SiC TO mode at the 838 nmwavelength. In FIG. 9, the ratio of the photoluminescence to the Ramansignal at LO mode (ratio (PL/LO)) of the No. 19 wafer of the secondembodiment is 5.1. Therefore, the silicon-vacancy density of the secondembodiment is about 5.1÷0.7=7.29 (×1E12 cm{circumflex over ( )}−3). Infact, the intensity and wavenumber of the peak of the LO mode aregreatly affected by the concentration of doping, and predicting thevacancy density of SiC through the ratio (PL/LO) is difficult. In orderto measure SiC with different resistivity, the photoluminescence signalof TO mode is used to measure the silicon-vacancy concentration becauseof its stability in different wafers and the same measurement area asphotoluminescence. In FIG. 9, the ratio of the photoluminescence to theRaman signal at the TO mode (ratio (PL/TO)) of the second embodiment is4.50. As a result, the silicon-vacancy density in 4H—SiC may becalculated by the following formula: density ofV_Si=PL/TO×7.29÷4.47=PL/TO×1.63. The PL/TO ratio is the peak ofcorresponding excitation light divided by the peak of the Ramanscattering at TO mode in the excitation spectrum (near 840 nm).Therefore, the silicon-vacancy density per unit lattice generatingsilicon-vacancy electroluminescence may be calculated (1PL/TO→1.630*10{circumflex over ( )}12/cm{circumflex over ( )}3).

The first embodiment was tested in the same method, and the maximumaverage vacancy density in the series was 3.26×1E12 cm{circumflex over( )}−3.

FIG. 11 is a schematic diagram of the PL/TO ratio of the firstembodiment. Taking the first embodiment as an example, nine measurementpoints are selected. The PL/TO ratio is shown in the figure, and thePL/TO ratio, silicon-vacancy concentration, and resistivity values ofthe nine measurement points (A, B, C, D, E, F, G, H, and I) are asfollows:

measurement silicon-vacancy resistivity values point PL/TO ratioconcentration (cm^(∧)−3) (ohm-cm) A 0.45 7.34E+11 1E11 B 0.43 7.01E+111E9 C 0.5 8.15E+11 1E11 D 0.32 5.22E+11 1E10 E 0.4 6.52E+11 1E11 F 0.641.04E+12 1E11 G 0.64 1.04E+12 1E11 H 0.65 1.06E+12 1E11 I 0.49 7.99E+111E10

FIG. 12 is a schematic diagram of the third embodiment of theapplication, and the diameter thereof is 60 mm. FIG. 13 is a schematicdiagram of the fourth embodiment of the application, and the diameterthereof is 120 mm. FIGS. 12 and 13 show the micro-pipe density (MPD). Inthe figure, the silicon carbide wafer is divided into multiple squares,and the numbers in the squares refer to the number of micro-pipes. Thenumber of micro-pipes in the third embodiment is 60. Dividing by thearea of the wafer, the micro-pipe density may be obtained as2.1/cm{circumflex over ( )}2. The number of micro-pipes in the fourthembodiment is 56. Dividing by the area of the wafer, the micro-pipedensity may be obtained as 0.5/cm{circumflex over ( )}2.

In the high-purity crystal growth system of the present application, bycontrolling the Si/C ratio and particle size distribution of thehigh-purity crystal growth raw material, and the crystal growthtemperature and time during the crystal growth process, the systembecomes a carbon-rich (C-rich) environment. In a state whereshallow-level conductive elements are scarce, the intrinsic defect ofsilicon vacancy may be generated in the crystal and the silicon-vacancyconcentration may be controlled. The intrinsic defect is used toincrease the resistivity of the crystal in order to make the wafer besemi-insulated.

The fifth embodiment illustrates growing a 6-inch single-crystal siliconcarbide bulk material by using the growth system of FIG. 1. Thissingle-crystal silicon carbide bulk material may be used as the rawmaterial for the crystal and wafer mentioned in the first to fourthembodiments. In other words, the crystal and wafer mentioned in thefirst to fourth embodiments may be processed from the bulk material ofthe present embodiment or from the bulk material obtained in a similarmethod to the present embodiment. For example, sublimate the rawmaterial of silicon carbide or react a gas-phase carbon source with asilicon source, and then deposit them on seed and grow into a siliconcarbide bulk material. When the deposition or growth time is short, thethickness of the bulk material may be 10 μm, 20 μm, or 30 μm, and theshape thereof is similar to a thin film. When the deposition or growthtime increases, the thickness of the bulk material gradually increasesto between 8 mm and 3 cm, and a large crystal is formed. The crystal maybe the crystal mentioned in the above embodiment. Further, the thicknessof the bulk material may be between 10 μm and 5 cm, wherein the thinneris called a thin film, and the thicker is called a crystal. Furthermore,the bulk material may also be processed into a wafer through asemiconductor process. The bulk material may be used as a raw materialfor the wafer or crystal of the above embodiment, but also as a rawmaterial for the silicon carbide powder, which will be further explainedbelow.

In the present embodiment, the semi-insulating single-crystal siliconcarbide bulk material is manufactured by the PVT method, and the growthprocess is performed in a graphite crucible in a high-temperature vacuuminduction furnace. In this way, a single crystal of 4H—SiC may beobtained. Specifically, the material used is high-purity silicon carbidepowder with a purity of 99.99% or more. The average particle size is 5mm to 20 mm. The initial silicon/carbon ratio is 1. After the crystalgrowing, the silicon/carbon ratio of the remaining material drops to0.85. The following are the process steps. First, place the siliconcarbide powder in a graphite container and introduce the silicon carbidepowder into the relatively hot end of the high-temperature vacuuminduction furnace. Then, place the seed in the relatively cold end ofthe high-temperature vacuum induction furnace. The seed may be a 4H—SiCsingle-crystal wafer with a diameter of 6-inch or 4H—SiC single-crystalingot with a diameter of 6-inch, and the thickness thereof is about 500μm. Fix the seed with a holder, and pump to remove the air and otherimpurities in the crucible system. In the heating process, add inert gasAr, and add hydrogen, methane, and ammonia as auxiliary gases. Heat theentire system by a heating coil to about 2200° C. and continually growfor up to 150 hours. The pressure is about 5 torr. Through the processconditions of the fifth embodiment, a 6-inch single-crystal siliconcarbide boule with a convex interface shape may be produced, and thecrystal growth rate may achieve 300 μm/hr.

It should be noted that the method mentioned in the present embodimentis only one of the methods for manufacturing semi-insulatingsingle-crystal silicon carbide bulk material. That is, thesemi-insulating single-crystal silicon carbide bulk material provided inthe present embodiment may be manufactured by other similar methods.More specifically, the semi-insulating single crystal silicon carbidebulk material may be obtained by a similar method such as physical vapordeposition (PVD) or chemical vapor deposition (CVD). For example, if thebulk material is manufactured by the chemical vapor deposition method,the process temperature should be lowered to 1000° C. under the same orsimilar parameters. If the bulk material is manufactured by the physicalvapor deposition method, the deposition rate should be dropped to about10 μm/hr under the same or similar parameters. In other words, comparedwith the PVT method, the same or similar semi-insulating silicon carbidebulk material as described in the fifth embodiment may be also obtainedthrough PVD, CVD, and other similar methods after adjusting thecorresponding parameters. Therefore, the semi-insulating single-crystalsilicon carbide bulk material claimed by the present application shouldnot be limited to the PVT method, and the semi-insulating single-crystalsilicon carbide bulk material obtained under the same or similarconditions or processes should fall within the scope of the presentapplication.

Refer to FIGS. 14 to 17, which are respectively the silicon-vacancyconcentration of each slice of the semi-insulating single-crystalsilicon carbide bulk material of the fifth embodiment of the presentapplication. As shown in the figure, a total of 13 slices are cut.Wherein the serial number of the slice closest to the seed is 1, and theserial number of the slice closest to the growth surface is 13. Takingthe slices numbered 1, 4, 8, and 13 as an example, as they approach theseed crystal to approach the growth surface, the silicon-vacancyconcentrations are 7.83E+11, 7.17E+11, 1.08E+12, and 5.38E+12. Themaximum strength, FWHM, PL/TO ratio, and silicon-vacancy concentrationare as follows:

maximum intensity FWHM PL/TO silicon-vacancy No. (G) (G) ratioconcentration (cm^(∧)−3)  1 12242 5.4283 0.48 7.824E+11  4 11671 6.39650.44  7.17E+11  8 16291 5.7617 0.66  1.08E+12 13  9255 5.0293 0.33 5.38E+12

The semi-insulating single-crystal silicon carbide bulk materialaccording to the above embodiment comprises one polytype single-crystal.The semi-insulating single-crystal silicon carbide bulk material hassilicon vacancy inside, wherein the silicon-vacancy concentration is atleast greater than 5E11 cm{circumflex over ( )}−3 and less than 5E13cm{circumflex over ( )}−3.

In one embodiment, the semi-insulating single-crystal silicon carbidebulk material according to the above embodiment has a thickness greaterthan or equal to 10 μm.

In one embodiment, the semi-insulating single-crystal silicon carbidebulk material according to the above embodiment has a thickness lessthan or equal to 3 cm.

In one embodiment, the semi-insulating single-crystal silicon carbidebulk material according to the above embodiment has a diameter greaterthan or equal to 90 mm.

In one embodiment, the semi-insulating single-crystal silicon carbidebulk material according to the above embodiment has a diameter less thanor equal to 200 mm.

In one embodiment, the semi-insulating single-crystal silicon carbidebulk material formed by the growth system according to the aboveembodiment has a resistivity greater than 1E7 ohm-cm.

In one embodiment, the semi-insulating single-crystal silicon carbidebulk material formed by the growth system according to the aboveembodiment comprises one polytype single-crystal selected from 3C, 4H,6H, and 15R polymorphs of silicon carbide, wherein the 4H polymorph isthe most preferred currently.

The semi-insulating single-crystal silicon carbide bulk material may beused in the biomedical field as “fluorescent micron silicon carbide” inaddition to being used as the raw material for the crystal and waferdescribed in the first to the fourth embodiments. More specifically,semi-insulating single-crystal silicon carbide has luminescencecharacteristics and may be used as a tracking detection target.Therefore, a silicon carbide powder will be provided in the following.The silicon carbide powder may be obtained by molding or refining withself-impacting, waterjet, or diamond processing any one of the bulkmaterial, crystal, or wafer of the above embodiments mentioned. Bypowdering silicon carbide bulk material, crystal, or wafer, the totalsurface area may be increased to improve the luminous effect.

Refer to FIGS. 18-21, which are schematic diagrams of the processing,the silicon-vacancy concentration of the residue, the silicon-vacancyconcentration of each slice of residue, and the relationship between thewavelength and the luminous intensity of the semi-insulatingsingle-crystal silicon carbide powder of the sixth embodiment of thepresent application. Generally, when the bulk material is being diced toa wafer, residual material 8 will be left. The residual material 8 maybe used to make the silicon carbide powder 9A and the powder 9B in thepresent embodiment.

In order to ensure the stable quality of the powder, EPR analysis may beperformed on the residual material 8 before the refinement. As shown inFIG. 19, the main defect in the residual material 8 is silicon vacancy,and the maximum silicon-vacancy concentration is 7.07E12 cm{circumflexover ( )}−3. In addition, the residual material 8 may be cut into slicesand the silicon-vacancy concentration analysis may be performed on theslices corresponding to different positions. Taking the growth system ofFIG. 1 as an example, a total of 5 slices are cut. Wherein the serialnumber of the slice closest to the seed is 1, and the serial number ofthe slice closest to the growth surface is 5, that is, the number on thehorizontal axis of FIG. 20. As shown in FIG. 20, the silicon-vacancyconcentrations of slice number 1 to slice number 4 are relativelysimilar, and the silicon-vacancy concentration of slice number 5 isdifferent from the aforementioned four slices. Therefore, in the actualproduction of powders, slices with numbers 1 to 4 are used forrefinement to obtain powders with similar properties. If slice number 5is used for refinement, a powder with a higher silicon-vacancyconcentration may be obtained, which may be applied for powderapplications that require higher intensity photoluminescence signals.

Next, in the present embodiment, cut the residual material 8 by diamondto obtain the powder 9A, and self-impact the residual material 8 toobtain the powder 9B. The particle size of the powder 9A and the powder9B may be between 1 micrometer and 500 micrometers, depending on theactual conditions of use. In the present embodiment, the value is about30 micrometers. Due to the different processing methods, the powder 9Aand the powder 9B may have different surface morphologies. Morespecifically, in the process of self-impacting, the powders collide witheach other to remove the sharp and rough surfaces, thereby reducing thepowder size. Therefore, the surface of powder 9B is smoother than thesurface of powder 9A. That is, the obtained powder 9B has low lightscattering. As shown in FIG. 21, when the fluorescence test is performedon the powder 9A and the powder 9B with the same particle size, thepowder 9B may have a better luminous intensity. Another reason for thehigh luminous intensity of the self-impacted powder may be that underthe anhydrous process, the powder surface has fewer hydration bonds orhydrogen-oxygen bonds and other adhesion or coating, which affects thelight-emitting efficiency.

In order to make the technical features of the present application moresimple and understandable, a manufacturing method of semi-insulatingsingle-crystal silicon carbide powder will be provided in the following.The semi-insulating single crystal silicon carbide bulk material is usedas a raw material in the manufacturing method to obtain semi-insulatingsingle-crystal silicon carbide powder. Further, the semi-insulatingsingle-crystal silicon carbide powder has a high silicon-vacancyconcentration greater than 5E11 cm{circumflex over ( )}−3. In this way,the semi-insulating single-crystal silicon carbide powder manufacturedby the manufacturing method may be applied in the biomedical field.

Refer to FIG. 22, which is a flow chart of the manufacturing method ofsemi-insulating single-crystal silicon carbide powder according to theseventh embodiment of the present application. As shown in the figure,the manufacturing method of semi-insulating single-crystal siliconcarbide powder includes:

Step S1: Provide a semi-insulating single-crystal silicon carbide bulkmaterial, wherein the semi-insulating single crystal silicon carbidebulk material has a first silicon-vacancy concentration, and the firstsilicon-vacancy concentration is greater than 5E11 cm{circumflex over( )}−3.

In one embodiment, the semi-insulating single-crystal silicon carbidebulk material used in step S1 may be the semi-insulating single-crystalsilicon carbide bulk material of the fifth embodiment. However, thepresent application is not limited to thereto. In other embodiments, thesemi-insulating single-crystal silicon carbide bulk material used instep S1 may also be a semi-insulating single-crystal silicon carbidebulk material with a diameter between 90 mm and 200 mm.

Step S2: Refine the semi-insulating single-crystal silicon carbide bulkmaterial to obtain a semi-insulating single crystal silicon carbidecoarse particle, wherein the semi-insulating single-crystal siliconcarbide coarse particle has a second silicon-vacancy concentration and afirst particle size. The silicon-vacancy concentration is greater than5E11 cm{circumflex over ( )}−3, and the first particle size is between50 μm and 350 μm.

In one embodiment, in step S2, the semi-insulating single-crystalsilicon carbide bulk material may be refined with a four-shaft crusher.More specifically, after 4.8 kg of semi-insulating single crystalsilicon carbide bulk material is refined by the four-axis crusher, about3.66 kg of semi-insulating single-crystal silicon carbide coarseparticle may be obtained. That is, the conversion efficiency (weight ofoutput/weight of input) refined by the four-shaft crusher is about 0.75.

Step S3: Self-impact the semi-insulating single-crystal silicon carbidecoarse particle to obtain a semi-insulating single-crystal siliconcarbide powder, wherein the semi-insulating single-crystal siliconcarbide powder has a third silicon-vacancy concentration and a secondparticle size. The third silicon-vacancy concentration is greater than5E11 cm{circumflex over ( )}−3, and the second particle size is between1 μm and 50 μm.

As described in the sixth embodiment, the powder obtained by the drymethod (i.e., self-impacting) has a smooth appearance. Therefore, thepowder obtained by the dry method has higher silicon-vacancy signalintensity than the powder obtained by the wet method (for example,diamond wire processing). More specifically, the silicon-vacancy signalintensity may differ by more than 1.5 times.

In addition to obtaining powders with higher silicon-vacancy signalintensity, the self-impacting method may also reduce the introduction ofimpurities or abrasives. Therefore, the powder obtained by theself-impacting method has a lower content of impurity, so that theproduct has a higher purity.

On the hand, water or solvent as a medium is unnecessary with theself-impacting method. Therefore, the generation of hydration bonds orhydrogen-oxygen bonds due to water or solvent during the refiningprocess may be prevented, resulting in agglomeration of the powder.Furthermore, compared with the wet method, in which subsequent drying isnecessary, the self-impacting method, in which subsequent drying isunnecessary, may also prevent hard agglomeration during the subsequentdrying, resulting in agglomeration of the powder.

As described above, in step S3, the semi-insulating single-crystalsilicon carbide coarse particle may be refined with a grinder. Afluidized bed jet milling is used in the grinder. Therefore, in the caseof grinding without other material, abrasive wear and tool contaminationmay be reduced.

In one embodiment, in step S3, the semi-insulating single crystalsilicon carbide coarse particle between 500 g and 1000 g may be used asthe raw material of the semi-insulating single-crystal silicon carbidepowder. For example, the weight of the semi-insulating single-crystalsilicon carbide coarse particle as the raw material may be 500 g, 600 g,700 g, 800 g, 1000 g, or a range of any combination of the above values.

In one embodiment, step S3 may be implemented at a temperature less than100° C. Specifically, in the process of self-impacting, cold air may beinput to prevent the temperature from rising, so as to preventagglomeration or chemical reaction of the semi-insulating single-crystalsilicon carbide powder due to the increase in temperature.

In one embodiment, step S3 may be implemented at a relative humidity ofless than 50%. Specifically, the relative humidity of the environmentmay be controlled during the self-impacting process to prevent thegeneration of hydration bonds or hydrogen-oxygen bonds due to waterduring the refining process, resulting in powder agglomeration.

In one embodiment, the self-impacting time of step S3 may be implementedfor 200 mins to 600 mins. Specifically, the particle size of the powderchanges in a curve with the time of self-impacting. When the time ofself-impacting is less than 200 minutes, the powder is still too coarse.On the other hand, when the time of self-impacting is over 600 minutes,the change rate of the particle size of the powder gradually slows down.Therefore, the self-impacting implemented for 200 mins to 600 mins mayhave higher efficiency, and the expected powder particle size (i.e., 5μm) may be obtained.

Refer to FIGS. 23 to 29, which are respectively a particle size analysisdiagram of the semi-insulating single-crystal silicon carbide coarseparticle and particle size analysis diagrams of the semi-insulatingsingle-crystal silicon carbide powder according to the eighth embodimentof the present application. The eighth embodiment is an experimentalresult of the semi-insulating single-crystal silicon carbide powdermanufactured by the manufacturing method of the seventh embodiment. Morespecifically, FIG. 23 is a particle size analysis diagram ofsemi-insulating single-crystal silicon carbide coarse particle used asraw material. In addition, FIGS. 24 to 29 are the particle size analysisdiagrams of six groups of semi-insulating single-crystal silicon carbidepowder obtained according to different process parameters. In thefollowing, “sample 1” to “sample 6” are used as representatives.

In the particle size analysis chart, d(0.1) means that 10% of theparticle have a particle size smaller than the present value, and 90% ofthe particles have a size larger than the present value. d(0.5) meansthat 50% of the particles are smaller than the present value, and 50% ofthe particles are larger than the present value. d(0.9) means that 90%of the particles are smaller than the present value, and 10% of theparticles are larger than the present value. Therefore, in the presentapplication, d(0.5) is used to represent the median particle size.

As shown in FIG. 23, the d(0.5) of the semi-insulating single-crystalsilicon carbide coarse particle is 345 μm. That is, the semi-insulatingsingle crystal silicon carbide coarse particle with a median particlesize of 345 μm is used as the raw material for self-impacting in thepresent embodiment. Furthermore, the semi-insulating single-crystalsilicon carbide coarse particle with a median particle size of 345 μm isrefined by self-impacting to obtain samples 1 to 6 in the presentembodiment. The analysis results are shown in FIGS. 24 to 29 and thefollowing table:

sample1 sample2 sample3 sample4 sample5 sample6 rotating 15000 1500015000 15000 15000 15000 speed (rpm) time 480 250 200 600 250 220 (min)input (g) 880 398 362 1090 470 400 output 677 306 279 837 360 307 (g)d(0.5) 5.39 5.19 5.547 4.918 5.288 5.825 diameter (μm)

As shown in the analysis results, when the self-impacting for obtainingsample 1 to sample 6 is implemented between 200 minutes and 600 minutes,the conversion efficiency is about 75%, and the median particle size ofthe powder is about 5 μm. That is, with the manufacturing methoddisclosed in the seventh embodiment of the present application, thesemi-insulating single-crystal silicon carbide powder as shown in theeighth embodiment may be obtained.

In summary, the present application provides a manufacturing method ofsemi-insulating single-crystal silicon carbide powder, which obtains asemi-insulating single-crystal silicon carbide powder with a smoothappearance, low impurity content, and stable particle size byself-impacting. The semi-insulating single-crystal silicon carbidepowder may be used in various fields (for example, as a fluorescentmaterial in the field of biomedicine).

A person of ordinary skill in the art will understand current and futuremanufacturing processes, method and step from the content disclosed insome embodiments of the present disclosure, as long as the current orfuture manufacturing processes, method, and step performs substantiallythe same functions or obtain substantially the same results as thepresent disclosure. Therefore, the scope of the present disclosureincludes the above-mentioned manufacturing process, method, and steps.

The above descriptions are only examples of this application and are notintended to limit this application. This disclosure may have variousmodifications and changes for a person of ordinary skill in the art. Anymodification, equivalent replacement, improvement, etc. made within thespirit and principle of this application shall be included in the scopeof the claims of this disclosure.

What is claimed is:
 1. A method for manufacturing method ofsemi-insulating single-crystal silicon carbide powder, comprising:providing a semi-insulating single-crystal silicon carbide bulk, whereinthe semi-insulating single-crystal silicon carbide bulk has a firstsilicon-vacancy concentration, and the first silicon-vacancyconcentration is greater than 5E11 cm{umlaut over ( )}−3; refining thesemi-insulating single-crystal silicon carbide bulk to obtain asemi-insulating single-crystal silicon carbide coarse particle, whereinthe semi-insulating single-crystal silicon carbide coarse particle has asecond silicon-vacancy concentration and a first particle diameter, thesecond silicon-vacancy concentration is greater than 5E11 cm{circumflexover ( )}−3, and the first particle diameter is between 50 μm and 350μm; self-impacting the semi-insulating single-crystal silicon carbidecoarse particle to obtain a semi-insulating single-crystal siliconcarbide powder, wherein the semi-insulating single-crystal siliconcarbide powder has a third silicon-vacancy concentration and a secondparticle diameter, the third silicon-vacancy concentration is greaterthan 5E11 cm{circumflex over ( )}−3, and the second particle diameter isbetween 1 μm and 50 μm.
 2. The method for manufacturing method ofsemi-insulating single-crystal silicon carbide powder according to claim1, the step of self-impacting the semi-insulating single-crystal siliconcarbide coarse particle is implemented with an amount between 500 g to1000 g of the semi-insulating single-crystal silicon carbide coarseparticle.
 3. The method for manufacturing method of semi-insulatingsingle-crystal silicon carbide powder according to claim 1, the step ofself-impacting the semi-insulating single-crystal silicon carbide coarseparticle is implemented at a temperature under 100° C.
 4. The method formanufacturing method of semi-insulating single-crystal silicon carbidepowder according to claim 1, the step of self-impacting thesemi-insulating single-crystal silicon carbide coarse particle isimplemented at a relative humidity under 50%.
 5. The method formanufacturing method of semi-insulating single-crystal silicon carbidepowder according to claim 1, the step of self-impacting thesemi-insulating single-crystal silicon carbide coarse particle isimplemented for 200 mins to 600 mins.
 6. The method for manufacturingmethod of semi-insulating single-crystal silicon carbide powderaccording to claim 1, the step of self-impacting the semi-insulatingsingle-crystal silicon carbide coarse particle is implemented with agrinding machine.
 7. The method for manufacturing method ofsemi-insulating single-crystal silicon carbide powder according to claim1, the step of refining the semi-insulating single-crystal siliconcarbide bulk is implemented with a quad shaft shredder.
 8. The methodfor manufacturing method of semi-insulating single-crystal siliconcarbide powder according to claim 1, the diameter of the semi-insulatingsingle-crystal silicon carbide bulk is greater than 90 mm.
 9. The methodfor manufacturing method of semi-insulating single-crystal siliconcarbide powder according to claim 1, the diameter of the semi-insulatingsingle-crystal silicon carbide bulk is smaller than or equal to 200 mm.